HRID1013120

反应详情

EQUATION

反应方程式

HRID 1013120 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

Add 2-(3-chloropropyl)-2-phenyl-[1,3]dioxolane (38 g, 168 mmol) and potassium phthalimide (34.2 g, 184.4 mmol) to DMF (80 mL) and stir for 40 min at 150° C. Cool the reaction to RT, dilute with water (1 L) and extract the mixture with a mixture of EtOAc (500 mL) and hexanes (500 mL) and DCM (2 L). Dry (sodium sulfate), concentrate and recrystallize the solid from hot ethanol (600 mL). Filter and dry the residue under vacuum to isolate the title compound as a white solid (47.62 g, 84%).

WORKUP

后处理

  1. temperatureCool
  2. customthe reaction to RT
  3. extractionextract the mixture
  4. additionwith a mixture of EtOAc (500 mL) and hexanes (500 mL) and DCM (2 L)
  5. dry with materialDry (sodium sulfate)
  6. concentrationconcentrate
  7. customrecrystallize the solid from hot ethanol (600 mL)
  8. filtrationFilter
  9. customdry the residue under vacuum